US966478A

US966478A - Orange sulfur dye and process of making same.

Info

Publication number: US966478A
Application number: US54169510A
Authority: US
Inventors: Alfred Schaarschmidt
Original assignee: Gesellschaft fuer Chemische Industrie in Basel CIBA
Current assignee: BASF Schweiz AG
Priority date: 1910-02-03
Filing date: 1910-02-03
Publication date: 1910-08-09
Anticipated expiration: 1927-08-09

Description

"UNIT D STAT P J S -PATENT OFFICE.

ALFRED, sonnnnscnmn'r, or BASEL, SWITZERLAND, nssrenon. TO 'socm'rY or vcrnancronn INDUSTRY IN BAsLnor BASEL, SWITZERLAND."

ORlANGE SULFUR DYE AND PROCESS OF MAKING.- SAME.

No Drawing.

Specification of Letters Patent.

Au .9 Application filed February a, 1910. a Serial No. muses-T Al llliABLfi COPY Pate 1910.

T 0 all whom it may concern:

Be it known I, ALFRED SCHAAR- SCHMIDT, a subjectofil f e King of Saxony, and resident of Basel, -witzerland, have invented new and "useful: Orange Sulfurized Vat Dyestuffs of-Ithe rAnthracene' Series and a Process of Making'Sa'me, of which the following is a full, clear, and exact specification. p a I According to the Un' States Letters Patent No. 899,845, datediiiseptember 29th, 1908, and No. 902,895,;da November 8d, 1908, orange'to yellow .yat? yestufi's are obtained by subjecting the ude dyestuffs made by melting Q-metliylfiiitghraquinone or omega-monochloro 2 methyianthraquinone wi-th sulfur at a temperature below 300 C.

to a treatment with a hypochlorite.

According to the presentinwention ora 'lge vat-dyestplfs are obtained byptreating the said crude dyestuffs with con furic acid-before the treatment-"with hypocnlorite. i

The following examples illustrate the invention, the parts being by weight.

Example 1: 30 parts ofthe crude dyestulf made by melting 1 part of Q-methylanthraquinone with 3 parts of sulfur at 250 3OO C. are introduced into 600 parts of surfuric acid of 66 Baum specific gravityand the mixture is heated, while stirring. for 3-;t hours in the oil bath at 1-l0l50 (1., this being the temperature of the bathfThe cooled mass is introduced into water and the brownish black flocks which separate are filtered and washed until neutral. To the paste thus obtained there is added, while stirring, first at ordinary temperature and finally while gently warming, a solution of sodium hypochlorite until the active chlorin reaction is permanent. ish-black color of the'paste is thus changed to orange brick red. After cooling, the

mixture. is filtered and the solid matter is washed, pressed and dried. The dyestufi' forms a brick red powder and yields, when treated with alkaline hydrosulfite solution, a

solution, become clear orange of excellent fastness-to washing, light and chlorin,

Example 2: 20 parts of the product made I by heating 1 part of omega-monochloro-Q mcthylanthraquinone with 3 .fur at 220230 I Y 300-400 parts of concentrated sulfuric acid The original brown-1 C. are introduced into and'the mixture is heated atthe temperature of the water bath, for 6 hours, while stirring. The mass is then introduced into water and the black brown product, separated by filtration, is treated in the manner described in Example 1 with a solutionlof sodium hypochlorite. The dyestufi' -thus obtainedhas properties silnilarc-to those of the dyestuff made according to Example 1.

With. respect to the treatment with hypo- .chlorite it is to be noted that the hypochlorite need not be previously formed; for the same result may be attained by suspending the dyestuft" which has been treated with sulfuric acid, in a solution of com mon salt and passing an electric current through the solution.

'hat Iclaimis:

1. The described process 'for the manufacture of orange sulfuri'z ed vat dyestuffs, which consists in-treating the crude dyestuffs obtained by melting Q-methylanthra quiu'one with sulfur at a temperature below 300 C. with concentrated sulfuric acid and then treating the resulting products with a hypochlorite.

The described process for the manufacture of orange sulfurized vat dyestuffs which consists in treating the crude dyestuffs obtained by melting omega1nonochloro-2- methylanthraquinone with sulfur at a temperature below 300 C; with concentrated sulfuric acid and then treating the resulting products with a hypochlorite.

3. As new products the vat-dyestuffs, obtainable by treating the crude dyestuffs obtained by melting iZ-methylanthraqninone with sulfur at a temperature below 300 C.

by exposure to air or by a treatment with a dilute hypochlbrite solution, become clear orange of excellent fastness to washing, lightandchlorin.

parts of sul-' at. As new products the Vat-dyestuffs. ob-

tainabl-e by treating the crude dyestuffs ob-- tainedz by melting omegaanonochloro-Q- methylanthmquinwe with sulfur at a; tem tiun, become clear orange of excellent fast- 10 petature below 300? C. with. concentrated ness' to washing, light and chlorin:

sulfuric acid and then treating the resulting In witness whereof I-have hereunto si ed gi'oduct with a .hypochlo'rit'e,constituting inmy name this 21st day of J anuary'191 in y state brick red powders and yieldmg, the presence oftwo subscribing wltnessesf' when treated with alkaline hydtosulfite solu- ALFRED SCHALARSCHMIDT. .tion red-brown vats dyeing cotton red- Witnesses: I i brown tints,'whieh by exposure .to air or by G120. GIFFORD,

,a' treatment with a dilute hypoehlorite so1u-. AMAND Bnrmm v t